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As depicted in Figure 1b, the deposited NPVG-2 film consists of vertically aligned graphene nanosheets with a significantly higher density compared to the undoped VG film. This higher density is maintained throughout the doping processes, as shown in Figure S1 (Supporting Information). Additionally, TEM images confirm the presence of exposed and highly extended graphene edges, with approximately five layers in the basal plane, as observed through HRTEM (Figure 1c,d). These findings indicate the excellent electrical properties of NPVG. Moreover, HRTEM images reveal distinct lattice fringes with different characteristic spacings in the circled region (Figure 1e,f). The fast Fourier transform (FFT) pattern extracted from the red rectangular area exhibits two sets of diffraction spots. The interplanar spacing of 0.354 nm corresponds to the (002) plane of graphene, while the spacing of 0.251 nm corresponds to the (111) plane of BP. This correspondence is further confirmed by inverse FFT (Figure 1g). Additionally, the interlayer spacing of the (002) plane in NPVG is larger than that of nitrogen-doped vertical graphene (0.345 nm) and graphene (0.335 nm), as shown in Figure S2. This confirms the successful incorporation of phosphorus and nitrogen atoms into the graphene structure, as heteroatom doping can modify the C-C hybridization and expand the layer separation [20]. Thus, it is suggested that the solid BP precursor dissociates in the plasma environment, contributing to both heteroatom doping and the introduction of BP crystal domains. High-angle annular dark-field STEM image (Figure 1i) and element mappings demonstrate the homogeneous distribution of nitrogen and phosphorus elements throughout the entire region (Figure 1f–h). Importantly, the NPVG film, with its well-aligned morphology and embedded BP crystal domain structure, provides advantages for redox catalysis in metal-air batteries. The ordered graphene nanosheets serve as effective pathways for ion transportation and accelerate charge transfer processes, thereby enhancing reaction kinetics at the electrode-electrolyte interface [15,21]. Furthermore, the BP crystal can catalyze the oxygen evolution reaction and enhance the overall electrocatalytic activity towards oxygen.